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Materials 2022, 15, 3956 where iP is peak current density (A/cm2); Co, A, and Do represent the concentration of the 9 of 11 αnFD v1 2 ip =0.4958nAFCo o (4) RT reactants (mol/cm3), work electrode area (1.95465 cm2), and diffusion coefficient (cm2/s), respectively. Figure 10. Fitting curves of the peak potential (Epc) and the logarithm scan rate (lnv). pc Figure 11 shows the square wave voltammetry curve of the NaCl-CaCl -TiO system. Figure 11 shows the square wave voltammetry curve of the NaCl-CaCl2-TiO2 system. Three obvious reduction peaks between −1.5 V and 0 V can be seen from the curve. The Three obvious reduction peaks between −1.5 V and 0 V can be seen from the curve. The first peak of process a and b is near −0.5 V, the second peak of process c is near −1.0 V, first peak of process a and b is near −0.5 V, the second peak of process c is near −1.0V, and and the third peak of process d is near −1.4 V, which is roughly the same as the reduction the third peak of process d is near −1.4 V, which is roughly the same as the reduction peak peak potential of the CV curve. The irreversible process in the reduction process is the potential of the CV curve. The irreversible process in the reduction process is the main main reason for a little shift of the reduction peak. Process d is a reversible process, so reason for a little shift of the reduction peak. Process d is a reversible process, so the rela- the relationship between the half-peak width and the electron transfer number can be tionship between the half-peak width and the electron transfer number can be expressed expressed in Equation (5) [28]. The electron transfer number in process d calculated by in Equation (5) [28]. The electron transfer number in process d calculated by Equation (5) Equation (5) is 2.324, approximately 2, which corresponds to reaction (13). The reduction is 2.324, approximately 2, which corresponds to reaction (13). The reduction process of process of TiO to titanium was further confirmed as TiO →Ti O →Ti O →TiO→Ti. 2 24723 TiO2 to titanium was further confirmed as TiO2→Ti4O7→Ti2O3→TiO→Ti. Materials2022,15,xFORPEERREVIEW RT E =3.52 RT 10 of 11 E =3.52 1/212 nF (5) nF (5) Figure 11. Square wave voltammetry curves of the NaCl-CaCl2-TiO2 system with 4 V/s scan rate. Figure 11. Square wave voltammetry curves of the NaCl-CaCl2-TiO2 system with 4 V/s scan rate. 4. Conclusions 4. Conclusions TitaniummetalwaspreparedbytheelectrochemicalreductioninNaCl-CaCl binary Titanium metal was prepared by the electrochemical reduction in NaCl-CaC2l2 binary moltensaltat1073K,andthereductionprocessofTiO totitaniumcanbesummarized 2 molten salt at 1073 K, and the reduction process of TiO2 to titanium can be summarized as TiO2→Ti4O7→Ti2O3→TiO→Ti. As an intermediate product in the deoxidation process of TiO2, CaTiO3 can be spontaneously generated among Ca2+, O2−, and TiO2 in the NaCl- CaCl2 system. The dissolution behavior of TiO2 showed that there is no chemical dissolu- tion of TiO2 in the NaCl-CaCl2 molten salt system at 1073 K. Electro-deoxidation thermo- dynamics and electrochemical studies further confirmed that the reduction of TiO2 to ti-PDF Image | Electrochemical Mechanism of Molten Salt Electrolysis
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